CN104697836A - TEM sample preparation method - Google Patents
TEM sample preparation method Download PDFInfo
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- CN104697836A CN104697836A CN201510144200.9A CN201510144200A CN104697836A CN 104697836 A CN104697836 A CN 104697836A CN 201510144200 A CN201510144200 A CN 201510144200A CN 104697836 A CN104697836 A CN 104697836A
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Abstract
The invention relates to the technical field of a semiconductor technology, and provides a TEM sample preparation method. Firstly, a protective layer of the same thickness deposits on a silicon substrate, thickness adjustment layers of different thicknesses deposit on corresponding sample preparation areas based on the protective layer, then ion beam reduction and cutting are carried out on TEM samples, and finally TEM samples with different thickness areas are formed. The TEM sample preparation method resolves the problem in the prior art that for different kinds of detection, samples of different thicknesses often need to be prepared. The technical personnel can conveniently and rapidly prepare samples with different thickness areas through the method.
Description
Technical field
The present invention relates to technical field of manufacturing semiconductors, particularly relate to the sample preparation methods of a kind of TEM (TransmissionElectronMicroscope transmission electron microscope).
Background technology
In semiconductor manufacturing industry, have various checkout equipment, wherein EM is the important tool becoming the pattern of the film of device, size and characteristic for test set.Conventional EM wraps TEM (Transmission ElectronMicroscope transmission electron microscope) and SEM (ScanningElectron Microscope scanning electron microscope).The principle of work of TEM is that the print that need detect is thinning in modes such as cutting, grinding, ion millings, then TEM sight chamber is put into, with the electron beam irradiation print that high pressure accelerates, print pattern is amplified, projects on screen, take a picture, then analyze, an outstanding advantages of TEM has higher resolution, the pattern of the very thin film of Observable and size.
In prior art, those skilled in the art utilize the method for transmission electron microscope (TEM) to observe sample, and described sample is generally utilization and utilizes the method for cross section grinding or flat focus ion beam (FIB) to carry out making formation to sample silicon substrate.Conventional use FIB method carries out method prepared by TEM sample to be had a variety of, but the thickness of single sample is all the same.But, the thickness requirement of various analysis purpose to sample is different, such as, TEM observation is roughly about 100nm to the thickness requirement of sample, and EDX (X-ray energy spectrometer) requires larger to thickness of sample, about about 300nm, EELS (electronic energy loss spectrometer) are then less to the thickness requirement of sample, below about 60 nanometers.Therefore, if need to carry out different observation to sample, the sample preparing multiple different-thickness is often needed.
In sum, how can prepare the sample with different-thickness region quickly and easily on single sample and become those skilled in the art's problem demanding prompt solution.
Summary of the invention
The object of the invention is to provide a kind of TEM sample preparation method that can prepare different-thickness region on same sample quickly and easily.
To achieve these goals, the invention provides a kind of TEM sample preparation method, comprising:
Step S1, provide silicon substrate, and on described silicon substrate, confirm the sample preparation region that at least two thin degree are different;
The protective seam of step S2, upper surface sedimentary facies stack pile in each sample preparation region;
The upper surface of step S3, the protective seam corresponding in each sample preparation region deposits the thickness regulating course of different preset thickness;
Step S4, repetition implementation step S3, until described thickness regulating course meets the requirements;
Step S5, described TEM sample to be carried out to ion beam thinning;
Step S6, on described silicon substrate to described thinning after TEM sample carry out cutting technique, and extract TEM sample.
Preferably, the material of described protective seam is metal, adopts the method for flat focus ion beam to prepare described protective seam.
Preferably, Pt or W is adopted to carry out the depositing operation of described protective seam as source metal.
Preferably, described thickness regulating course is identical with the material of described protective seam.
Preferably, the method for flat focus ion beam is adopted to prepare described thickness regulating course.
Preferably, be under the condition of 30kv at voltage, employing electric current is the Ga ion beam of 50pA ~ 1000pA, carries out the cutting technique of TEM sample in focused ion beam equipment.
Preferably, the thickness range of described protective seam is 100 ~ 1000nm.
Preferably, the thickness range of described thickness regulating course is 100nm ~ 1000nm.
The invention provides a kind of TEM sample preparation method; first the protective seam of sedimentary facies stack pile on a silicon substrate; the thickness regulating course of corresponding each sample preparation area deposition different-thickness on the basis of protective seam; then the thinning and cutting of ion beam is carried out to TEM sample, final form the TEM sample with different-thickness region.The invention solves for different detections in prior art, often need the problem of the sample preparing multiple different-thickness, those skilled in the art adopt the method can prepare the sample with different-thickness region quickly and easily.
Accompanying drawing explanation
Fig. 1 is the FB(flow block) of TEM sample preparation method in the present invention;
Fig. 2 to Fig. 5 by TEM sample preparation method of the present invention embodiment the cross-sectional view of formation TEM sample.
Embodiment
For making content of the present invention clearly understandable, below in conjunction with Figure of description, content of the present invention is described further.Certain the present invention is not limited to this specific embodiment, and the general replacement known by those skilled in the art is also encompassed in protection scope of the present invention.Secondly, the present invention's detailed statement that utilized schematic diagram to carry out, when describing example of the present invention in detail, for convenience of explanation, schematic diagram, should in this, as limitation of the invention not according to general ratio partial enlargement.
Above-mentioned and other technical characteristic and beneficial effect, will in conjunction with the embodiments and accompanying drawing 1 to Fig. 5 TEM sample preparation method of the present invention is described in detail.Fig. 1 is the FB(flow block) of TEM sample preparation method in the present invention; Fig. 2 to Fig. 5 by TEM sample preparation method of the present invention embodiment the cross-sectional view of formation TEM sample.
Refer to Fig. 1, Fig. 1 is the FB(flow block) of TEM sample preparation method in the present invention; In the present embodiment, the invention provides a kind of TEM sample preparation method, comprise the following steps:
Step S1, provide silicon substrate, and confirm the sample preparation region that at least two thin degree are different on a silicon substrate;
The protective seam of step S2, upper surface sedimentary facies stack pile in each sample preparation region;
The upper surface of step S3, the protective seam corresponding in each sample preparation region deposits the thickness regulating course of different preset thickness;
Step S4, repetition implementation step S3, until thickness regulating course meets the requirements;
Step S5, TEM sample to be carried out to ion beam thinning;
Step S6, on a silicon substrate cutting technique is carried out to the TEM sample after thinning, and extract TEM sample.
Below in conjunction with specific embodiment, technical scheme of the present invention is described in detail.In order to technical scheme of the present invention is described better, incorporated by reference to the TEM sample method for making cross-sectional view of the one embodiment of the present invention shown in Fig. 2-Fig. 5.
First, refer to Fig. 2, silicon substrate 10 is provided, and on silicon substrate 10, confirm the sample preparation region 20 that at least two thin degree are different; Wherein, the position in sample preparation region 20 and quantity can be determined according to actual conditions.
Then, refer to Fig. 3, at the protective seam 30 of the upper surface sedimentary facies stack pile in each sample preparation region 20; Wherein, the material of protective seam 30 is preferably metal, Pt or W can be adopted to carry out the depositing operation of protective seam 30 as source metal, and preferably use the method for flat focus ion beam to prepare protective seam 30, the thickness range of protective seam 30 is preferably 100 ~ 1000nm.
Then, refer to Fig. 4, deposit the thickness regulating course 40 of different preset thickness at the upper surface of the protective seam 30 of each sample preparation region 20 correspondence, can repeat to implement this step, until thickness regulating course 40 meets the requirements; Wherein, preferably adopt the method for flat focus ion beam to prepare thickness regulating course 40, thickness regulating course 40 is preferably identical with the material of protective seam 30, and the thickness range of thickness regulating course 40 is preferably 100nm ~ 1000nm.
Again then, ion beam carries out to TEM sample thinning; Ion beam is slow in the sample preparation region cutting speed that metal level is thicker, defines the sample preparation region of different-thickness.
Finally, refer to Fig. 5, on silicon substrate 10, cutting technique carried out to the TEM sample 50 after thinning, and extract TEM sample 50.Wherein, be under the condition of 30kv at voltage, preferably employing electric current is the Ga ion beam of 50pA ~ 1000pA, carries out the cutting technique of TEM sample 50, and is proposed out, carry out TEM detection in focused ion beam equipment.
In sum; the invention provides a kind of TEM sample preparation method; first the protective seam 30 of sedimentary facies stack pile on silicon substrate 10; the thickness regulating course 40 of corresponding each sample preparation area deposition different-thickness on the basis of protective seam 30; then the thinning and cutting of ion beam is carried out to TEM sample, final form the TEM sample 50 with different-thickness region.The invention solves for different detections in prior art, often need the problem of the sample preparing multiple different-thickness, those skilled in the art adopt the method can prepare the sample with different-thickness region quickly and easily.
The above is only the description of the preferred implementation of invention; should be understood that; due to the finiteness of literal expression; and objectively there is unlimited concrete structure; for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.Any simple modification, equivalent variations and modification, all still belong in the scope of technical solution of the present invention protection.
Claims (8)
1. a TEM sample preparation method, is characterized in that, comprising:
Step S1, provide silicon substrate, and on described silicon substrate, confirm the sample preparation region that at least two thin degree are different;
The protective seam of step S2, upper surface sedimentary facies stack pile in each sample preparation region;
The upper surface of step S3, the protective seam corresponding in each sample preparation region deposits the thickness regulating course of different preset thickness;
Step S4, repetition implementation step S3, until described thickness regulating course meets the requirements;
Step S5, described TEM sample to be carried out to ion beam thinning;
Step S6, on described silicon substrate to described thinning after TEM sample carry out cutting technique, and extract TEM sample.
2. TEM sample preparation method according to claim 1, is characterized in that, the material of described protective seam is metal, adopts the method for flat focus ion beam to prepare described protective seam.
3. TEM sample preparation method according to claim 2, is characterized in that, adopts Pt or W to carry out the depositing operation of described protective seam as source metal.
4. TEM sample preparation method according to claim 2, is characterized in that, described thickness regulating course is identical with the material of described protective seam.
5. TEM sample preparation method according to claim 4, is characterized in that, adopts the method for flat focus ion beam to prepare described thickness regulating course.
6. TEM sample preparation method according to claim 1, is characterized in that, is under the condition of 30kv at voltage, and employing electric current is the Ga ion beam of 50pA ~ 1000pA, carries out the cutting technique of TEM sample in focused ion beam equipment.
7., according to the arbitrary described TEM sample preparation method of claim 1 ~ 6, it is characterized in that, the thickness range of described protective seam is 100 ~ 1000nm.
8., according to the arbitrary described TEM sample preparation method of claim 1 ~ 6, it is characterized in that, the thickness range of described thickness regulating course is 100nm ~ 1000nm.
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| CN105092330A (en) * | 2015-08-12 | 2015-11-25 | 上海华力微电子有限公司 | Method for preparing TEM sample |
| CN105241718A (en) * | 2015-10-13 | 2016-01-13 | 武汉新芯集成电路制造有限公司 | Transmission electron microscope (TEM) sample preparation method |
| CN106908290A (en) * | 2017-02-16 | 2017-06-30 | 中国科学院合肥物质科学研究院 | The preparation method of holography observation transmission electron microscope sample |
| CN112881439A (en) * | 2021-03-09 | 2021-06-01 | 洪启集成电路(珠海)有限公司 | OLED TEM sample preparation method and OLED TEM sample |
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| CN112881439A (en) * | 2021-03-09 | 2021-06-01 | 洪启集成电路(珠海)有限公司 | OLED TEM sample preparation method and OLED TEM sample |
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